CN102539374B - Method for measuring coal gas component and calorific value - Google Patents

Method for measuring coal gas component and calorific value Download PDF

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CN102539374B
CN102539374B CN201110435862.3A CN201110435862A CN102539374B CN 102539374 B CN102539374 B CN 102539374B CN 201110435862 A CN201110435862 A CN 201110435862A CN 102539374 B CN102539374 B CN 102539374B
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CN102539374A (en
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刘志强
熊友辉
何涛
石平静
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Sifang Optoelectronic Co., Ltd.
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WUHAN CUBIC OPTOELECTRONICS CO Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/22Fuels, explosives
    • G01N33/225Gaseous fuels, e.g. natural gas
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/14Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
    • G01N7/18Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by allowing the material to react

Abstract

The invention discloses a method for measuring coal gas components and calorific values, which comprises the following steps: measuring the volume concentrations of CO, CO2, CH4, CnHm in coal gas by non-dispersive infrared technology and by selecting narrowband optical filters with center wavelength CWL/half width bandwidth HWBP being respectively 4.66+/-0.05 microns/90+/-5 nm, 4.26+/-0.05 microns/120+/-5 nm, 7.85+/-0.05 microns/180+/-5 nm, 3.46+/-0.05 microns/120+/-5 nm; measuring the volume concentrations of H2 by a thermal-conductive gas sensor; measuring the volume concentrations of O2 by a electrochemical sensor, correcting the CnHm measured result by the CH4 measured value, correcting the H2 measured result by the CO2 and CH4 measured values so as to obtain accurate CO, CO2, CH4, CnHm, H2, O2 contents in the coal gas components, and automatically calculating the calorific value. The invention realizes rapid and accurate measurement of the components and calorific value of multi-component coal gas in one apparatus. Compared with traditional methods, the invention has obvious advantages with respect to apparatus production cost, accuracy, rapidity, and the like.

Description

A kind of for measuring the method for gas composition and calorific value
Technical field
The present invention relates to a kind of method of measuring gas composition and calorific value, the method that particularly can be revised void fraction.
Background technology
Coal gasification is the important component part of China's Coal Chemical Industry, particularly under the condition of China's oil resource growing tension, seems more important.The detection analysis of gas composition is the prerequisite of gasification furnace optimal control, is also the important parameter of other operations of Coal Chemical Industry industry.Blast furnace, converter, coke oven and glass, the industrial circles such as pottery also often need to carry out the detection of gas composition.
Austenite gas analysis is as a kind of chemical formula manual analyzing device of classics, have low price, easy to operate, keep in repair the advantages such as easy, at the gas composition analysis field, be widely used always.But the method is a kind of manual operation, and precision is low, speed is slow, can not adapt to the industrial expansion needs.Chromatograph is promoted in recent years, but chromatograph detects after need to being separated gas again, is difficult to realize real-time online, and needs a plurality of chromatographic columns of configuration and use carrier gas.Infrared gas analyzer uses for many years in China, but conventional art often can only be analyzed one-component in a set of analytical instrument, or two components, and the instrument of the type is not only expensive, and maintenance is complicated.In addition for the CH in coal gas 4the measurement meeting because of the existence phase mutual interference of other hydrocarbons, can't Measurement accuracy.H in coal gas 2, O 2volumetric concentration can not be measured by the NDIR method, often adopts TCD to measure H 2volumetric concentration, adopt ECD to measure O 2volumetric concentration, and the CH in coal gas 4with other C nh mthere is the phase mutual interference, CH 4, CO 2disturb H Deng meeting 2.In patent CN201886002U, the inventor has researched and developed a kind of gas analysis system, and this system can reach single injected sampling by chromatographic technique and analyze the CO in coal gas 2, O 2, CO, CH 4, H 2, C 2h 4, C 2h 6etc. the purpose of gas concentration, but this system needs carrier gas, measurement when analyzing gas composition, be discontinuous measurement, also can't realize on-the-spot portable measurement.Be subject in addition the restriction of chromatographic column, for C 3h 8, C 4h 10can't measure Deng material, therefore can not obtain calorific value of gas accurately.In patent CN101750439A, the inventor provides a kind of modified single channel hydrogen gas sensor, effectively improve and optimize by the hydrogen gas sensor physical arrangement to based on thermal conduction principle, reduced to greatest extent the baseline wander that environment and self temperature variation are brought, but this sensor is to adopt the H2 in N2 to be demarcated, if other components, particularly CO in coal gas except H2 2, CH 4after variation, density of hydrogen just needs to revise just can obtain accurate concentration.Owing to there is no CO 2, CH 4data, so revise and can't complete.In patent US2008011952A1, ABB (Asea Brown Boveri Ltd) company has proposed a kind of Non-Dispersive Infra-red (NDIR) gas analyzer, this analyser adopts the Non-Dispersive Infra-red (NDIR) technology, a plurality of gas sensors can be set, reach the purpose of simultaneously measuring multiple asymmetric gas concentration, every kind of gas sensor has a measurement passage and a contrast passage can improve measuring accuracy so simultaneously.But this classification is analysed instrument and is usually adopted the narrow band pass filter of 3.4um left and right to measure CH 4, C nh m, under the coal gas measurement environment, due to C nh mwith CH 4the phase mutual interference very large, therefore can't measure the CH in the main source of calorific value of gas 4and C nh m.Can not configure in addition the TCD thermal conductivity sensor in this instrument simultaneously and measure the concentration of hydrogen, even the independent instrument that the type is installed uses as combined instrument, also there is no CO 2, CH 4deng gas to H 2the correction of measuring, can't directly obtain the calorific value of coal gas more.
In sum, domestic also do not have at present instrument can be in an instrument the various compositions in Measurement accuracy coal gas, particularly contribute the CH of energy 4, C nh m, CO, H 2composition.Therefore be necessary to work out a kind of calorific value that can measure various compositions in coal gas simultaneously and calculate coal gas, and can effectively get rid of the method for disturbing between gas.
Summary of the invention
Problem and shortcoming that the present invention exists in order to overcome above-mentioned prior art, the invention provides a kind of more accurate for measuring the method for gas composition and calorific value.The method is compared with above-mentioned existing method of testing, has advantages of following: the present invention can measure the various kinds of coal gas composition simultaneously; By preferred NDIR narrow band pass filter parameter, reduce the interference between gas with various; Select 3.46 mum wavelength optical filters to measure C nh m, other hydrocarbons all can be converted to C 3h 8, be convenient to the calculating of calorific value of gas; According to the void fraction of gained, calculate the calorific value of coal gas; Use the analytical instrument manufacturing cost of this method for 1/3 of traditional combustion method caloric value instrument, only have 1/10 of mass spectrometer, analysis speed is that tradition is chromatographic more than 30 times.
Technical scheme of the present invention is:
A kind of for measuring the method for gas composition and calorific value, adopt thermal conductance gas sensor (TCD) to measure H 2volumetric concentration T h2, adopt electrochemical sensor (ECD) to measure O 2volumetric concentration, calculate the calorific value of coal gas by measured and revised various void fractions, it is characterized in that comprising the following steps:
(1) adopt Non-Dispersive Infra-red (NDIR) (NDIR) technology, measure CO, CO in coal gas 2, CH 4, C nh mvolumetric concentration; Count respectively T cO, T cO2, T cH4, T cnHm;
(2) using formula R cnHm=T cnHm-A * T cH4revise CH 4to C nh minterference, wherein, A is undetermined coefficient, T cnHm, T cH4the C that NDIR records successively nh m, CH 4volumetric concentration;
(3) using formula R h2=T h2-a * (T cH4+ R cnHm)-b * T cO2revise H 2the measured value of volumetric concentration, wherein T h2tCD actual measurement H 2volumetric concentration, T cH4and T cO2respectively NDIR actual measurement CH 4and CO 2volumetric concentration, R cnHmrevised C nh mvolumetric concentration, a, b are undetermined coefficient;
(4) use heat value formula Q=T cO* 12.64+R h2* 18.79+T cH4* 35.88+R cnHm* 93.18 calculate calorific value of gas, wherein T cOand T cH4for actual measurement volumetric concentration, R h2and R cnHmfor revised void fraction.
Adopt NDIR principle Measurement accuracy CH 4, selected narrow band pass filter parameter is that centre wavelength CWL/ half peak bandwidth HWBP is 7.85 ± 0.05 μ m/180 ± 5nm.
Adopt the NDIR principle to measure C nh m, selected narrow band pass filter parameter is that centre wavelength CWL/ half peak bandwidth HWBP is 3.46 ± 0.05 μ m/120 ± 5nm.
Adopt the NDIR principle to measure CO, selected narrow band pass filter parameter is that centre wavelength CWL/ half peak bandwidth HWBP is 4.66 ± 0.05 μ m/90 ± 5nm.
Adopt the NDIR principle to measure CO 2, selected narrow band pass filter parameter is that centre wavelength CWL/ half peak bandwidth HWBP is 4.26 ± 0.05 μ m/120 ± 5nm.
Method of the present invention is compared with above-mentioned existing method of testing, has advantages of following: the present invention can measure the various kinds of coal gas composition simultaneously; By preferred NDIR narrow band pass filter parameter, reduce the interference between gas with various; Select 3.46 mum wavelength optical filters to measure C nh m, other hydrocarbons all can be converted to C 3h 8, be convenient to the calculating of calorific value of gas; According to the void fraction of gained, calculate the calorific value of coal gas; Use the analytical instrument manufacturing cost of this method for 1/3 of traditional combustion method caloric value instrument, only have 1/10 of mass spectrometer, analysis speed is that tradition is chromatographic more than 30 times.
The accompanying drawing explanation
Fig. 1 is gas composition analysis principle figure.
Fig. 2 is CO, CO 2, CH 4infrared absorption pattern figure.
Fig. 3 is the mutual interference figure of hydrocarbon in 3.3 μ m left and right.
Fig. 4 is CH 4infrared absorption pattern figure.
Embodiment
Below in conjunction with case, the present invention will be described in detail:
Case 1: gasification of biomass 6 component gas analysis meters
1, various gas optical filter parameters and air chamber length, the selection of range
At first according to CO, CO 2infrared absorption pattern, as Fig. 2, the absorption peak of CO at 4.66 μ m places is not subject to the interference of CO2, therefore the absorption peak of CO2 at 4.26 μ m places do not disturbed by CO, selects respectively narrow band pass filter that parameter is 4.66 μ m/90nm, 4.26 μ m/120nm as CO, CO 2the detector optical filter, reference channel is chosen as 3.91 μ m, the CO air chamber length is chosen as 43mm, CO 2air chamber length is chosen as 2mm, the CO that the CO gas sensor that the making range is 40% and range are 30% 2gas sensor.
Then according to CH 4, C 2h 6, C 3h 8, C 4h 10infrared absorption pattern, as Fig. 3, Fig. 4, be to eliminate C nh mto CH 4therefore the interference of absorption peak, do not select the absorption peak that parameter is 3.3 μ m places, and select the absorption peak at 7.85 μ m places, selects narrow band pass filter that parameter is 7.85 μ m/180nm as CH 4the detector optical filter, reference channel is chosen as 3.91 μ m, CH 4air chamber length is chosen as 68mm, the CH that the making range is 20% 4gas sensor.
According to C nh minfrared absorption pattern, as Fig. 3, C between 3.3--3.5 μ m nh mabsorption peak is arranged, in order to reduce CH 4to C nh minterference, should avoid CH 4absorption peak, select centre wavelength between 3.35--3.5 μ m, by the different optical filters in 3.35--3.5 μ m scope, tested, find to select narrow band pass filter that parameter is 3.46 μ m/120nm as C nh mthe detector optical filter, can use C 3h 8represent C nh m(C nh muse C 3h 8demarcate).Reference channel is chosen as 3.91 μ m, C nh mair chamber length is chosen as 43mm, the C that the making range is 5% nh mgas sensor.Test data is as table 1.
The impact of table 1:C1~C5 on 3.46 μ m sensors
Figure BDA0000123835010000041
Table 2:C nh mthe Lower heat value coefficient
The gas title Lower heat value coefficient (MJ/m 3) Calorific value coefficient ratio (C nH m/C 3H 8)
C 2H 6 64.35 0.69
C 3H 8 93.18 1.00
C 4H 10 123.16 1.32
C 5H 12 156.63 1.68
By contrast table 1 and table 2, can find out C nh mthe volumetric concentration scale-up factor and the calorific value coefficient ratio that at the sensor of the detector made that adopts 3.46 μ m/120nm narrow band pass filters, record are very approaching, so can use C 3h 8represent C nh mcarry out computing heating value.
Finally, adopt the H that known fabrication techniques range is 20% thermal conductance TCD type 2sensor, range is 25% galvanochemistry ECD type O 2sensor.
2, measure various void fractions
Use NDIR to measure CO, CO 2, CH 4, C nh m, reading is designated as respectively T cO, T cO2, T cH4, T cnHm.
Use TCD to measure H 2volumetric concentration, be designated as T h2.
Use ECD to measure O 2volumetric concentration, be designated as T o2.
3, void fraction correction and calorific value calculation.
(1) pass through CH 4to C nh mrevised.
Due to CH 4to C nh mcertain interference is arranged, treat to calculate C by calibration curve nh mmeasurement result (T cnHm) time, also need according to CH 4volumetric concentration (T cH4) to T cnHmrevised, obtained revised C nh mvolumetric concentration (R cnHm).
For revising CH 4the impact that CnHm is measured, pass into CH to the gasification of biomass 6 component gas analysis meters of present case 4calibrating gas, calibrating gas volumetric concentration and measurement result are as table 3:
Table 3:CH 4calibrating gas volumetric concentration and measurement result
Figure BDA0000123835010000061
By analyzing data, can obtain following correction formula:
R CnHm=T CnHm-A×T CH4
The data substitution formula of table 3 can be drawn to A=0.02868
So R cnHm=T cnHm-A * T cH4=T cnHm-0.02868 * T cH4.
(2) revise H 2volumetric concentration.
For adopting TCD to measure H 2volumetric concentration, due to CH 4, CO 2with H 2demarcate the Balance Air N of use 2on the relatively hot conductance, larger difference is arranged, in Table 4, so CH 4, CO 2to H 2measurement result has certain interference; C nh malthough on thermal conductivity with N 2variant, but its content in coal gas is only CH 41/5 left and right, therefore do not consider; And CO, O 2thermal conductivity and N 2thermal conductivity difference very little, do not consider yet.So only need to be according to CH 4, CO 2measurement result T cO2, T cH4to H 2measurement result T h2revised, obtained revised H 2volumetric concentration (R h2).
Table 4: the thermal conductivity of gas with various
Figure BDA0000123835010000062
Figure BDA0000123835010000071
For revising CH 4, CO 2to H 2the impact of measurement result, pass into CH to the gasification of biomass 6 component gas analysis meters of present case 4, CO 2calibrating gas, calibrating gas volumetric concentration and measurement result are as table 5:
Table 3:CH 4, CO 2to H 2impact
Figure BDA0000123835010000072
By analyzing data, can obtain following correction formula:
R H2=T H2-a×T CH4-b×T CO2
The data substitution formula of table 5 can be drawn to a=0.13989; B=-0.11026
So R h2=T h2-a * T cH4-b * T cO2.=T H2-0.13989×T CH4+0.11026×T CO2
(3) calculate calorific value of gas
According to the above gas concentration obtained, by T cO, T cH4, R cnHmand R h2the substitution formula
Q=T cO* 12.64+R h2* 18.79+T cH4* 35.88+R cnHm* 93.18 obtain the calorific value of coal gas.
Wherein, Q unit is MJ/m 3, 12.64,18.79,35.88 and 93.18 are respectively CO, H 2, CH 4, C nh mthe Lower heat value coefficient, unit is MJ/m 3.
Present case has designed that a kind of CO range is 40%, CO 2range is 30%, CH 4range is 20%, C nh mrange is 5%, H 2range is 20%, O 2the 6 component gas analysis meters that range is 25%, be adapted at air gas, Biomass Air Gasification, blast furnace, a plurality of sector applications such as heat absorption type, heat release formula carbide feed generator for thermal treatment.Case 2: biomass pyrolytic, coking 6 component gas analysis meters
1, the selection of various gas air chamber lengths, range
Accomplice example 1 aspect the optical filter selection of NDIR infrared gas sensor design.At the air chamber design aspect: the CO air chamber length is chosen as 43mm, the CO gas sensor that to make range be 40%; CO 2air chamber length is chosen as 3mm, the CO that the making range is 20% 2gas sensor; CH 4air chamber length is chosen as 34mm, the CH that the making range is 50% 4gas sensor; C nh mair chamber length is 20mm, the C that the making range is 10% nh mgas sensor;
Adopt the H that known fabrication techniques range is 75% 2sensor; The O that the making range is 25% 2sensor.
2, measure various void fractions
Use NDIR to measure CO, CO 2, CH 4, C nh m, reading is designated as respectively T cO, T cO2, T cH4, T cnHm.
Use TCD to measure H 2volumetric concentration, be designated as T h2.
Use ECD to measure O 2volumetric concentration, be designated as T o2.
3, void fraction correction and calorific value calculation.
(1) pass through CH 4to C nh mrevised.
For revising CH 4to C nh mthe impact of measuring, pass into CH to biomass pyrolytic, the coking 6 component gas analysis meters of present case 4calibrating gas, calibrating gas volumetric concentration and measurement result are as table 6:
Table 6:CH 4calibrating gas volumetric concentration and measurement result
Figure BDA0000123835010000081
Figure BDA0000123835010000091
By analyzing data, can obtain following correction formula:
R CnHm=T CnHm-A×T CH4
The data substitution formula of table 6 can be drawn to A=0.02837
So R cnHm=T cnHm-A * T cH4=T cnHm-0.02837 * T cH4.
(2) revise H 2volumetric concentration.
For revising CH 4, CO 2to H 2the impact of measurement result, pass into CH to biomass pyrolytic, the coking 6 component gas analysis meters of present case 4, CO 2calibrating gas, calibrating gas volumetric concentration and measurement result are as table 7:
Table 7:CH 4, CO 2to H 2impact
Figure BDA0000123835010000092
Figure BDA0000123835010000101
By analyzing data, can obtain following correction formula:
R H2=T H2-a×T CH4-b×T CO2
The data substitution formula of table 7 can be drawn to a=0.14097; B=-0.11091
So R h2=T h2-a * T cH4-b * T cO2.=T H2-0.14097×T CH4+0.11091×T CO2
(3) calculate calorific value of gas
According to the above void fraction obtained, by T cO, T cH4, R cnHmand R h2the substitution formula
Q=T cO* 12.64+R h2* 18.79+T cH4* 35.88+R cnHm* 93.18 obtain the calorific value of coal gas.
Wherein, Q unit is MJ/m 3, 12.64,18.79,35.88 and 93.18 are respectively CO, H 2, CH 4, C nh mthe Lower heat value coefficient, unit is MJ/m 3.
Present case has designed that a kind of CO range is 40%, CO 2range is 20%, CH 4range is 50%, the CnHm range is 10%, H 2range is 75%, O 2the 6 component gas analysis meters that range is 25%, be adapted at a plurality of sector applications such as mixed gas in coking, biomass pyrolytic, destructive distillation, iron and steel.
Above embodiment is used for illustrative purposes only, but not limitation of the present invention, person skilled in the relevant technique, without departing from the spirit and scope of the present invention, can also make various conversion or modification, therefore all technical schemes that are equal to also should belong to category of the present invention, should be limited by each claim.

Claims (3)

1. one kind for measuring the method for gas composition and calorific value, adopts thermal conductance gas sensor TCD to measure H 2volumetric concentration T h2, adopt electrochemical sensor ECD to measure O 2volumetric concentration is characterized in that comprising the following steps:
(1) adopt Non-Dispersive Infra-red (NDIR) NDIR technology, measure CO, CO in coal gas 2, CH 4, C nh mvolumetric concentration; Count respectively T cO, T cO2, T cH4, T cnHm; Wherein, adopt NDIR principle Measurement accuracy CH 4, selected narrow band pass filter parameter is that centre wavelength CWL/ half peak bandwidth HWBP is 7.85 ± 0.05 μ m/180 ± 5 nm; Adopt the NDIR principle to measure C nh m, selected narrow band pass filter parameter is that centre wavelength CWL/ half peak bandwidth HWBP is 3.46 ± 0.05 μ m/120 ± 5 nm;
(2) using formula R cnHm=T cnHm-A * T cH4revise CH 4to C nh minterference, wherein, A is undetermined coefficient, T cnHm, T cH4the C that NDIR records successively nh m, CH 4volumetric concentration;
(3) using formula R h2=T h2-a * (T cH4+ R cnHm)-b * T cO2revise H 2the measured value of volumetric concentration, wherein T h2tCD actual measurement H 2volumetric concentration, T cH4and T cO2respectively NDIR actual measurement CH 4and CO 2volumetric concentration, R cnHmrevised C nh mvolumetric concentration, a, b are undetermined coefficient;
(4) use heat value formula Q=T cO* 12.64+ R h2* 18.79+T cH4* 35.88+R cnHm* 93.18 calculate calorific value of gas, and wherein Q unit is MJ/m 3, T cOand T cH4for actual measurement volumetric concentration, R h2and R cnHmfor revised void fraction.
2. according to claim 1 for measuring the method for gas composition and calorific value, it is characterized in that: adopt the NDIR principle to measure CO, selected narrow band pass filter parameter is that centre wavelength CWL/ half peak bandwidth HWBP is 4.66 ± 0.05 μ m/90 ± 5 nm.
3. according to claim 1 for measuring the method for gas composition and calorific value, it is characterized in that: adopt the NDIR principle to measure CO 2, selected narrow band pass filter parameter is that centre wavelength CWL/ half peak bandwidth HWBP is 4.26 ± 0.05 μ m/120 ± 5 nm.
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PCT/CN2012/080795 WO2013091399A1 (en) 2011-12-22 2012-08-30 Coal gas component and calorific value measurement method
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